Acetic Acid → 1-Acetyl-5-carbomethoxy-7-chloro-4-methoxy-1,2-dihydroindole

HRID 2074002노트

반응식

HRID 2074002 반응식
[C:1]([N:4]1[C:12]2[C:7](=[C:8]([O:18][CH3:19])[C:9]([C:14]([O:16][CH3:17])=[O:15])=[CH:10][C:11]=2[Cl:13])[CH:6]=[CH:5]1)(=[O:3])[CH3:2].C(O)(=O)C>[Pt].CO>[C:1]([N:4]1[C:12]2[C:7](=[C:8]([O:18][CH3:19])[C:9]([C:14]([O:16][CH3:17])=[O:15])=[CH:10][C:11]=2[Cl:13])[CH2:6][CH2:5]1)(=[O:3])[CH3:2]

참가 물질

5

반응물 2

HCID 176Acetic AcidHCID 104931031-Acetyl-5-carbomethoxy-7-chloro-4-methoxyindole

생성물 1

HCID 105649501-Acetyl-5-carbomethoxy-7-chloro-4-methoxy-1,2-dihydroindole

시약·촉매·용매 2

HCID 23939Platinum촉매HCID 887Methanol용매

실험 절차

The mixture of the indole of step 8 above (0.9 g) and Pt-C (0.2 g), acetic acid and MeOH (100 ml) is stirred under H2 at 1 atm. pressure for 48 hours. The catalyst is filtered (celite), the filtered material is washed (MeOH) and the reaction mixture and methanol washings are evaporated. The residue is diluted with CH2Cl2, washed with saturated NaHCO3, dried (MgSO4) and evaporated affording a colorless, semicrystalline material which is determined to be the desired compound by NMR. M.P. 107°-109° C.

후처리

  1. filtrationThe catalyst is filtered (celite)
  2. washthe filtered material is washed (MeOH)
  3. customthe reaction mixture and methanol washings are evaporated
  4. additionThe residue is diluted with CH2Cl2
  5. washwashed with saturated NaHCO3
  6. dry with materialdried (MgSO4)
  7. customevaporated
  8. customaffording a colorless, semicrystalline material which

출처 및 근거

ORD 기록
ord-be1d126f7a2a4da2bef77007ed389b1e
출처 데이터셋
uspto-grants-1990_04
특허 번호
US04920219

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